TITLE

Microstructure Examination of Steel

OBJECTIVES

To observe the constituents and structure of metals and their alloys by means of an optical
microscope.

INTRODUCTION

Microscopic examinations could satisfy many purposes and one of the key persistence of it in
materials engineering is examining defects in materials. Defects in a material determines
important properties and performing microstructure examinations helps to develop relations
between the microstructure of the material and its properties. Defects and imperfections
are crucial factors and there are many types of defects. The material defect this
particular experiment will focus on is an area defect, which is called grain boundary
defect. It is an interfacial defect where there is boundaries separating different crystallographic
orientations in polycrystalline materials. The purpose of the experiment was to inspect the
microstructure, the shape and size of the grains for different samples. The experiment was
performed with optical microscope which is not as precise as electronic microscopes but is very
easy to use and the results can be achieved much faster.
Metallography can be defined as the visual study of the constitution and structure of materials.
Metallographic examination can be broadly categorized into two types namely, macroscopic
examinations and microscopic examinations. Macroscopic examinations refer to the observations
carried out at a magnification of X10 of less. Microscopic examinations, on the other hand, refer
to the examination of the structure at a magnification greater than X10. Microscopic
examinations, depending on the nature of information to be extracted, can be accomplished using
an Optical Microscope (up to X2000) or Scanning Electron Microscope (up to X50000) or a
Transmission Electron Microscope (up to X500000). For most of the routine purposes in optical
microscope is used to obtain firsthand information on the geometric arrangement of the grains
and phases in a material. In order to retain the information visualized using the microscope,
microstructural details are often recorded on a 35mm film or a Polaroid film. The photograph
thus obtained, revealing the microstructural details, taken at a magnification of greater than X10
is known as a photomicrograph. Maintaining a record of the microstructural studies in the form
of photomicrographs is a common practice employed by research scholars and leading
laboratories all over the world.
The study of microstructural details is important due to its correlation with ensuring the
mechanical properties of the material. As an example, if material A exhibits more homogeneous
and refined microstructure than material B, it may very well be anticipated that material A will
exhibit better room temperature properties when compared to material B.
In order to metallographically examine a specimen, it is essential to learn the various steps that
required preparing it. The following section briefly describes the various steps involved in the
metallographic preparation of the sample.
The basic operation outlining the metallographic preparation of the specimens is as follows:

Selection of the Size of the Specimen: The selection of the grain size of the specimen is dependent
on the nature of material and the information to be gathered. Normally, the linear dimensions may
vary from 5mm to 3mm while the thickness is kept lower than the linear dimensions.

Mounting the Specimen: Mounting of the specimen is normally carried out, if the specimen does
not permit convenient handling. Plastic mounting carried out by placing the specimen in a plastic or
rubber mold face down, filling the mold with mounting grade of plastic and allowing it to dry for a
few hours. The plastic mounting is carried out such that the surface to be examined is exposed on
one side of the plastic mount.

Rough Grinding: Rough grinding is carried out on the emery belt surface in order to round off the
corners, if necessary and to remove deep scratches from the surface.

Fine Grinding: Fine grinding involves rubbing of the specimen against the silicon carbide powders
bonded on to specially prepared papers. There are various grit sizes of silicon carbide papers and the
ones normally used are 400 grit, 600 grit and 1000 grit papers. These papers are mounted on a flat
surface. Grinding involves holding the specimens downwards on the abrasive paper followed by
rubbing in forward and backward directions until the surface is covered with an even pattern of fine
scratches. The process is repeated with successively finer grade papers (increase in grit number).
With each change of paper, the specimen should be turned trough 900 to facilitate the observation of
the disappearance of the previous scratch marks. In addition, at every new stage the specimen and
equipment should be washed of grit and dirt from the preceding grinding.

Rough Polishing: This stage involves the polishing of the specimen surface on a rotating wheel
using alumina or diamond abrasive with a particle size of about 5 microns. Polishing aids include
diamond particle suspension or alumina powder suspension. In the polishing stage, the specimen is
moved around the wheel in the direction opposite to the wheel itself. This ensures a uniform
polishing action.

Fine Polishing: This stage involves the removal of very fine scratches and the thin disorted layer
remaining from the rough polishing stages. Fine polishing is usually carried on a polishing wheel
using fine alumina particles with an average size of less than 1 micron (normally 0.5 micron size is
used). Fine polishing, if properly carried out, yields a scratch free surface ready for etching.
Etching: Etching is carried out on the properly dried specimen obtained from fine polishing step.
Etching involves chemically treating the specimen surface using a mild acidic or alkaline solution.
The etchant differentially attacks various microstructural features as a result of their different
chemical affinities. This differential attack leads to a non-similar reflection of light into the
objective lens leading to the generation of contrast between the various microstructural features.
After etching is successfully carried out, the specimen can be taken to the optical microscope for
microstructural examination.

Microscopy can give information concerning a material’s composition, previous treatment and
properties. Particular features of interest are:
1. Grain size
2. Phases present
3. Chemical homogeneity
4. Distribution of phases
5. Elongated structures formed by plastic deformation

Grain size determination: Grain size may be determined using an intercept method described below;
Straight lines, all of the same length, are drawn through several photomicrographs that show the
grain structure. The grains intersected by each line segment are counted; the line length is then
divided by an average of the number of grains intersected, taken over all the line segments.

Figure 1 shows a typical Fe-Fe3C metastable phase diagram. The various phases in this phase
diagram which may be of interest to us can be defined as follows:

 Ferrite (α-iron): a solid solution of carbon in iron having a maximum carbon content of
about 0.022%.
 Austenite (-iron): a solid solution of carbon in iron formed at high temperatures
containing a maximum carbon content of about 2.11%
 Cementite (Fe3C) a compound of carbon and iron, having a chemical formula of Fe3C
and a carbon content 6.7%
 Pearlite (α+Fe3C): a two phase mixture that exists with an average carbon content of
0.77%. Pearlite has a lamellar structure.
 Figure 1: Fe-Fe3C Phase Diagram
( adopted from http://www.slideshare.net/drsjose/fe-c-diagram)

THEORY
The properties of metals highly depend on their structures. The internal structures determine how
materials perform under a given application. The effects of most industrial processes applied to
metals to control their properties can be explained by studying their rnicrostructures. The branch
of materials science dealing with microscopic examination of metals is called Metallography.

The most common method used to examine the structures of materials is optical technique. A
specimen about 20 mm on an edge is cut from the metal to be examined. In some cases where the
subject is small or unhandy like razor blade, it is embedded in a plastic case which is called
“mounting”. A mirror polish is produced on one face of the specimen by grinding on
successively fine emery (sand) papers and polishing on revolving cloth wheels with fine
abrasives such as diamond or alumina powder. To reveal the structural details such as grain
boundaries, phases and inclusions, this polished surface is etched with chemical solutions. The
etchant attacks various parts of the specimen at different rates and reveals the structure. A
metallographic microscope is used to examine the microstructure.

MATERIALS AND APPARATUS

 Steel Specimen
 Optical Microscope
PROCEDURE

 The samples used as specimen in this experiments are: Steel after annealing and
quenching.
 At first the specimen was mounted on a glass slide and in order to make sure that the
surface of the sample is level with horizontal plane moulding clay is used.
 Using the specimen press the specimen is pressed on to the moulding
 Then the glass slide mounted specimen is placed on the holder/clamp on the optical
microscope.
 After the specimen is placed the zooming scale is changed and simultaneously the
specimen is viewed using the microscope.
 When better image is received from the optical microscope the observations can be made
CALCULATIONS

According to the microstructure sketch,

9.9 cm = 400 µm

 Number of straight lines = 6

 Length of a straight line = 8 cm
 Converted length of a straight line = (8/9.9) X 400µm
= 323.232µm
 Total length of the straight lines = 323.232µm x 6 = 1939.393 µm
 Total number of grains counted = 77

Average grain size = [(323.232) x6]\77 µm

= 25.186µm
RESULTS

The experiment of microstructure examination involves important analysis regarding grain

boundary defects of the crystal structures. The grain boundary’s size is calculated using a very
systematic process. The shape of the image is also an important factor. Using the given image of
grain boundary, the size calculation is demonstrated. As the image is equiaxed the process of
calculation will be as following.
First straight lines of same length are drawn. More than 5 straight lines should be drawn. The
lines that lie inside a grain boundry is taken as a ½. The grains intersected by each line segment
are counted; the line length is then divided by an average of the number of grains intersected, taken
over all the line segments. Then using the formula the grain size is calculated.

Grain size = Total length of the lines

Number of grains intersected

Grain Size = 25.186 µm

CONCLUSION

The microstructure examination experiment provided an important information of any

crystalline structure, may it be metallic or non-metallic. The observation through optical
microscope gave a clearer understanding of the grains. The grain boundary and size
determination made in the experiment demonstrates the practical way of calculating grain size
from SEM image without using the grain size data from ASTM. After observing sample of steel
the observatory comparisons satisfied the objective of the experiment.
There may be residual effects of these processes and treatments, inclusion or
contaminants that can be explained by microstructure analysis and microscopic examination. In
many cases, the investigation centers on the correlation between the resulting microstructure and
the material properties.

REFERENCES

1. Engineering Metallurgy- Part I by R. A. Higgins

2. Callister, William D. Jr. “Interfacial Defects.” Materials Science and Engineering. 7th ed.
3. Eng. D.D. Wanasinghe “Phase Diagrams.” MT101 Class,SLIIT. 19th Aug,2015.
4. R. Balasubramaniam, Callister’s Materials Science and Engineering – 2nd Edition